反应详情

[Ethoxycarbonyl[2-(5-methylfuran-2-yl)ethyl]amino]-acetic acid (0.17 g) prepared in the step 5 was dissolved in 3.5 mL of methylene chloride, then 0.12 g of thionyl chloride and 1 drop of DMF were added thereto and the mixture was heated to reflux for 2 hours. After the reaction solution was cooled, it was diluted with 5 mL of methylene chloride, then 0.18 g of aluminum chloride was added thereto and the mixture was heated to reflux again for 30 minutes. After the reaction solution was cooled, it was poured over 50 mL of ice water, the organic layer was separated, washed with water and a saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom in vacuo. The residue was purified by silica gel column chromatography to give 0.07 g of the objective compound as yellow liquid.

1. temperaturethe mixture was heated
2. temperatureto reflux for 2 hours
3. temperatureAfter the reaction solution was cooled
4. temperaturethe mixture was heated
5. temperatureto reflux again for 30 minutes
6. temperatureAfter the reaction solution was cooled
7. customthe organic layer was separated
8. washwashed with water
9. dry with materiala saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate
10. customthe solvent was evaporated
11. customThe residue was purified by silica gel column chromatography